CN107893216A - A kind of method corrected quartzy monitoring method and prepare broadband anti-reflection film deposition errors - Google Patents

A kind of method corrected quartzy monitoring method and prepare broadband anti-reflection film deposition errors Download PDF

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CN107893216A
CN107893216A CN201710944000.0A CN201710944000A CN107893216A CN 107893216 A CN107893216 A CN 107893216A CN 201710944000 A CN201710944000 A CN 201710944000A CN 107893216 A CN107893216 A CN 107893216A
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thickness
film
layer
reflection film
monitoring
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CN107893216B (en
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程鑫彬
王占山
董思禹
焦宏飞
鲍刚华
张锦龙
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Tongji University
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/54—Controlling or regulating the coating process
    • C23C14/542—Controlling the film thickness or evaporation rate
    • C23C14/545—Controlling the film thickness or evaporation rate using measurement on deposited material
    • C23C14/547—Controlling the film thickness or evaporation rate using measurement on deposited material using optical methods
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24—Vacuum evaporation
    • C23C14/28—Vacuum evaporation by wave energy or particle radiation
    • C23C14/30—Vacuum evaporation by wave energy or particle radiation by electron bombardment

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
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  • Health & Medical Sciences (AREA)
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  • Physical Vapour Deposition (AREA)
  • Length Measuring Devices By Optical Means (AREA)

Abstract

The present invention relates to a kind of method corrected quartzy monitoring method and prepare broadband anti-reflection film deposition errors, this method comprises the following steps：1) design monitoring thickness, prepares a four layer series, the four layer series include made of high-index material double-layer filmses of two kinds of thickness and made of low-index material two kinds of thickness double-layer filmses；2) by the reverse inverting of the four layer series to preparation and linear fit, the film gauge variation of high-index material and low-index material is obtained；3) filming parameter of broadband anti-reflection film to be prepared is modified with the film gauge variation of identical material.Compared with prior art, the present invention can effectively correct deposition errors and to improve spectrum property, simple to operate and universality strong so that broadband anti-reflection film can produce extensively in practice.

Description

A kind of method corrected quartzy monitoring method and prepare broadband anti-reflection film deposition errors
Technical field
Field of optical films of the present invention, deposition is corrected in quartzy monitoring method prepares broadband anti-reflection film more particularly, to one kind The method of error.
Background technology
With the fast development of Modern Optics Technology, the requirement to optical thin film correlation properties also improves constantly.Remove Apply the Laser Films in the low-loss AR film and laser fusion device in gravitational wave detecting device, image width Also have become the emphasis of people's care with the wider and more complicated optical thin film of this optical characteristics of anti-reflection film.Generally, broadband The number of plies of anti-reflection film is more, and each thickness degree differs, and comprising compared with film layer, these bring very big to the actual preparation of film Difficulty.Deposition errors caused by due to monitoring technology can have a strong impact on the spectral characteristic of broadband anti-reflection film, therefore how real The Accurate Calibration of existing film actual deposition thickness, and accurately amendment is to improve broadband anti-reflection film spectrum by the deposition errors of film layer The key factor of energy.
Quartzy monitoring method is a kind of method of wide variety of monitoring film thickness, suitable for most of precipitation equipment With the monitoring of various thickness thin films, have the advantages that easy to install, setting is simple, signal is easily processed and can automatically controlled.When When quartzy monitoring method being used alone in electron beam evaporation deposition equipment preparing broadband anti-reflection film, due to precision controlled by the method Limitation, film layer actual (real) thickness can have larger error, and the optical characteristics to broadband anti-reflection film causes strong influence.And Non-linear relation is presented with its thickness in the relative error of film layer, and thicknesses of layers is smaller, and relative error is bigger, and this is for deposition errors Accurate acquisition and amendment cause great difficulty.
The method of directly amendment deposition errors is that the thickness error of various film layers is directly obtained using transmission electron microscope, Measuring accuracy is high, reliable results, but this method has testing expense costliness, and test process can damage to sample surfaces Problem.The method of indirect amendment deposition errors is the reverse method of inversion based on sample spectra, but due to relative error and film Non-linear relation between thickness, and broad-band transparence-increased membrane system it is complicated and the problem of cause spectrum multi-solution, these can have a strong impact on The reliability of reverse inversion result, leads to not accurately obtain real deposition errors.So far still without it is a kind of reliable, efficiently, And the strong method of non-destructive universality can accurately obtain and correct quartzy monitoring method and prepare broadband anti-reflection film deposition errors Method.
The content of the invention
It is an object of the present invention to overcome the above-mentioned drawbacks of the prior art and provide one kind corrects quartz monitoring The method that method prepares broadband anti-reflection film deposition errors.
The purpose of the present invention can be achieved through the following technical solutions：
A kind of method corrected quartzy monitoring method and prepare broadband anti-reflection film deposition errors, this method comprise the following steps：
1) design monitoring thickness, prepares a four layer series, and the four layer series are included two kinds made of high-index material The double-layer filmses of thickness and made of low-index material two kinds of thickness double-layer filmses；
2) by the reverse inverting of the four layer series to preparation and linear fit, high-index material and low-refraction are obtained The film gauge variation of material；
3) filming parameter of broadband anti-reflection film to be prepared is modified with the film gauge variation of identical material.
Further, the step 1) is specially：
The four layer series are coated with substrate using ion beam assisted depositing technique, the prison with quartzy monitor by setting Control the deposition of thickness monitoring film.
Further, the step 2) is specially：
201) the Optical transmission spectrum curve using the four layer series that spectrophotometer measurement is prepared in normal incidence, lead to The reverse inverting to the curve of spectrum is crossed to obtain the actual deposition thickness of every layer film；
202) monitoring thickness of two kinds of materials per tunic and actual deposition thickness are determined two directly as data point respectively Line equation, the intercept of each equation is film gauge variation of the respective material in deposition process, specifically,
Determine that linear equation y=ax+b, wherein slope a are Tooling factor with two data points corresponding to every kind of material, cut It is film gauge variation of the respective material in film deposition process away from b.
Further, in the four layer series, the thickness range of thick-layer film is 100~150nm, the thickness of thin film Scope is 5~15nm.
Further, in the step 3), the filming parameter of broadband anti-reflection film to be prepared is modified specially： The film gauge variation of identical material is subtracted on the basis of thickness initial design values per layer film, realizes and thickness error is carried Preceding amendment.
The present invention provides a kind of broad-band transparence-increased membrane preparation method, and this method comprises the following steps：
Set the thickness initial design values per layer film in broadband anti-reflection film to be prepared；
The thickness is initially set according to the method that the described quartzy monitoring method of amendment prepares broadband anti-reflection film deposition errors Evaluation is modified, and the monitoring thickness of quartzy monitor is used as using correction result；
It is coated with substrate using ion beam assisted depositing technique, with the deposition of quartzy monitor monitoring film, is obtained Required broad-band transparence-increased membrane sample.
The present invention designs and prepares four tunics that two kinds of materials of a high low-refraction needed for broadband anti-reflection film form System；The thin film deposition thickness monitored using quartzy monitor, referred to as monitors thickness；And the method determination for passing through reverse inverting is thin Film actual (real) thickness；Monitoring thickness of two kinds of materials per tunic and actual (real) thickness are determined into linear equation as data point respectively, side The intercept of journey is thickness deviation of every kind of material in deposition process；When being formally coated with broadband anti-reflection film, identical material is utilized The thickness deviation of material is corrected in advance to filming parameter, it is ensured that the optical characteristics of broadband anti-reflection film reaches preparation and required, significantly Improve the transmissivity of broadband anti-reflection film.
Compared with prior art, the invention has the advantages that：
1st, expense is low and destroys small：The present invention obtains film actual (real) thickness deviation by reverse inversion method, and right with this Filming parameter is modified, relative to directly by transmission electron microscope test method, the cycle is short, cost greatly reduce and Do not damage film surface；
2nd, it is easy to operate：Only need to be coated with the four layer series of two kinds of materials used in a broadband anti-reflection film, every kind of material respectively wraps Containing a thin layer and a thick-layer, the membrane system without being coated with all thickness of broadband anti-reflection film can be completed to correct；
3rd, accuracy is high：Using the reverse method of inversion as foundation, four layer series structure is employed, it is inversely anti-to reduce complicated membrane system Drill middle spectrum multi-solution to have a strong impact on result, the transmissivity for the broadband anti-reflection film that the inventive method coats, which has, significantly to be carried Height, in 450~900nm gamut internal transmission factors, the entirety of minimum point 98% brings up to more than 99% before amendment.
Brief description of the drawings
Fig. 1 is the schematic flow sheet of modification method of the present invention；
Fig. 2 is broad-band transparence-increased membrane system design drawing；
Fig. 3 is broadband anti-reflection film theoretical transmission spectroscopic data figure；
Fig. 4 is TiO2/SiO2The reverse inverting schematic diagram of four layer series transmitted spectrum；
Fig. 5 is TiO2The linear equation result schematic diagram that two data points are obtained according to inversion result and determined；
Fig. 6 is SiO2The linear equation result schematic diagram that two data points are obtained according to inversion result and determined；
Fig. 7 is broad-band transparence-increased film theory, the transmittance spectra data figure before error correction and after error correction.
Embodiment
The present invention is described in detail with specific embodiment below in conjunction with the accompanying drawings.The present embodiment is with technical solution of the present invention Premised on implemented, give detailed embodiment and specific operating process, but protection scope of the present invention is not limited to Following embodiments.
As shown in figure 1, the present invention provides a kind of method corrected quartzy monitoring method and prepare broadband anti-reflection film deposition errors, should Method comprises the following steps：
1) design monitoring thickness, is coated with a four layer series, four tunic using ion beam assisted depositing technique on substrate System includes made of high-index material double-layer filmses of two kinds of thickness and two kinds of thickness made of low-index material Double-layer filmses, the deposition with quartzy monitor by the monitoring thickness monitoring film of setting.
In the four layer series, the thickness range of thick-layer film is 100~150nm, the thickness range of thin film for 5~ 15nm。
2) by the reverse inverting of the four layer series to preparation and linear fit, high-index material and low-refraction are obtained The film gauge variation of material, specifically：
201) the Optical transmission spectrum curve using the four layer series that spectrophotometer measurement is prepared in normal incidence, lead to The reverse inverting to the curve of spectrum is crossed to obtain the actual deposition thickness of every layer film；
202) monitoring thickness of two kinds of materials per tunic and actual deposition thickness are determined two directly as data point respectively Line equation, the intercept of each equation is film gauge variation of the respective material in deposition process.
3) filming parameter of broadband anti-reflection film to be prepared is modified with the film gauge variation of identical material, Specially：The film gauge variation of identical material is subtracted on the basis of the thickness initial design values of every layer film, is realized to thickness Spend the amendment in advance of error.
Broadband anti-reflection film closer to goal-selling can be obtained by above-mentioned modification method.
In this implementation exemplified by preparing the broadband anti-reflection film of 450~900nm wave band normal incidences, specific implementation step is as follows：
(1) according to experiment demand, 450~900nm wave bands are being designed on a quartz substrate just first by thin film design software Incident broad band anti-reflection film；Select TiO2And SiO2As high low refractive index film material, choose quartz and be used as substrate, film structure As shown in Fig. 2 H represents TiO2Film layer, L represent SiO2Film layer, most thin layer and thickest layer are respectively 5nm and 130nm in membrane system；Fig. 3 Give the transmitted spectrum of Theoretical Design：Normal incidence 450~900nm wavelength regions rate is more than 99.7%.
(2) same quartz of choosing is used as substrate, designs one in addition by TiO2And SiO2The four layer series of composition, specifically set It is calculated as TiO2(10nm)/SiO2(10nm)/TiO2(100nm)/SiO2(140nm), every kind of material respectively includes a thin layer in membrane system With a thick-layer, its spectral band applied is 400~900nm.
(3) TiO is prepared using ion beam assisted depositing technique2And SiO2Four layer series；High-index material uses during plated film Ti3O5Particle uses SiO as target, low-index material2Ring is as target；In deposition process, the thickness and deposition speed of film Rate is controlled by quartzy monitor, TiO2Sedimentation rate isSiO2Sedimentation rate isIon gun oxygen flow is 50sccm, argon flow amount 10sccm, voltage 900V, electric current 1000mA；Plated film terminates rear sample and is slowly annealed in vacuum chamber Room temperature, and sample is taken out after aging 12 hours and is put into drying cupboard preservation.
(4) TiO being prepared using spectrophotometer Cary5000 measurements2And SiO2Four tunic samples 400~ 900nm Optical transmission spectrum curve, by obtaining the actual deposition thickness of every layer film to the reverse inverting of transmittance graph, Selected 400~900nm spectral regions covering and close to the design wave band of broadband anti-reflection film, at the same comprising visible ray with it is closely red Outside, the accuracy of reverse inverting is added, can lift the precision of error correction, acquiescence TiO used during inverting2And SiO2Film Optical constant accurately and reliably, then chooses the actual (real) thickness of random thickness error model fitting film, is fitted four obtained tunics The actual deposition thickness of system is TiO2(11.45nm)/SiO2(12.65nm)/TiO2(101.42nm)/SiO2(142.62nm)。
(5) it is directed to TiO in four layer series2And SiO2Respective double-layer filmses, respectively using the monitoring thickness of every tunic as horizontal seat Mark, using actual deposition thickness of the film on sample as ordinate, determine the linear equation of every kind of material with two data points, two Intercept in linear equation is thickness deviation of the respective material in film deposition process.Specifically, corresponding to every kind of material Two data points determine linear equation y=ax+b, when wherein slope a represents indirect monitoring, film deposit thickness on a monitor Ratio between the deposit thickness on sample, referred to as Tooling factor, intercept b are thickness of the respective material in film deposition process Spend deviation.
Fig. 4 gives reverse fitting schematic diagram of the four layer series based on transmission spectrum curve, and Fig. 5 and Fig. 6 sets forth The TiO determined therefrom that2And SiO2The result of linear equation, the crystal oscillator thickness that abscissa provides are to monitor thickness, wherein TiO2With SiO2Thickness deviation be respectively 1.45nm and 2.65nm.
(6) according to the TiO of gained2And SiO2Thickness deviation, deviation size is cut in the design of broadband anti-reflection film, from And error is modified in advance, broadband anti-reflection film is prepared by step (3) the identical method, you can obtain optical characteristics Excellent broad-band transparence-increased membrane sample, the actual transmission spectrum curve of its spectrophotometer measurement as shown in fig. 7, with uncorrected width The curve of spectrum with anti-reflection film compares, and is brought up in 450~900nm gamuts internal transmission factor from minimum point 98% is overall More than 99%.
Preferred embodiment of the invention described in detail above.It should be appreciated that one of ordinary skill in the art without Creative work can is needed to make many modifications and variations according to the design of the present invention.Therefore, all technologies in the art Personnel are available by logical analysis, reasoning, or a limited experiment on the basis of existing technology under this invention's idea Technical scheme, all should be in the protection domain being defined in the patent claims.

Claims (6)

  1. A kind of 1. method corrected quartzy monitoring method and prepare broadband anti-reflection film deposition errors, it is characterised in that this method include with Lower step：
    1) design monitoring thickness, prepares a four layer series, and the four layer series include two kinds of thickness made of high-index material Double-layer filmses and made of low-index material two kinds of thickness double-layer filmses；
    2) by the reverse inverting of the four layer series to preparation and linear fit, high-index material and low-index material are obtained Film gauge variation；
    3) filming parameter of broadband anti-reflection film to be prepared is modified with the film gauge variation of identical material.
  2. 2. the method that the quartzy monitoring method of amendment according to claim 1 prepares broadband anti-reflection film deposition errors, its feature exist In the step 1) is specially：
    The four layer series are coated with substrate using ion beam assisted depositing technique, it is thick by the monitoring of setting with quartzy monitor Spend the deposition of monitoring film.
  3. 3. the method that the quartzy monitoring method of amendment according to claim 1 prepares broadband anti-reflection film deposition errors, its feature exist In the step 2) is specially：
    201) the Optical transmission spectrum curve using the four layer series that spectrophotometer measurement is prepared in normal incidence, by right The reverse inverting of the curve of spectrum obtains the actual deposition thickness of every layer film；
    202) monitoring thickness of two kinds of materials per tunic and actual deposition thickness are determined into two straight line sides as data point respectively Journey, the intercept of each equation is film gauge variation of the respective material in deposition process.
  4. 4. the method that the quartzy monitoring method of amendment according to claim 1 prepares broadband anti-reflection film deposition errors, its feature exist In in the four layer series, the thickness range of thick-layer film is 100~150nm, and the thickness range of thin film is 5~15nm.
  5. 5. the method that the quartzy monitoring method of amendment according to claim 1 prepares broadband anti-reflection film deposition errors, its feature exist In in the step 3), being modified specially to the filming parameter of broadband anti-reflection film to be prepared：In the thickness of every layer film The film gauge variation of identical material is subtracted on the basis of initial design values, realizes the amendment in advance to thickness error.
  6. 6. a kind of broad-band transparence-increased membrane preparation method, it is characterised in that this method comprises the following steps：
    Set the thickness initial design values per layer film in broadband anti-reflection film to be prepared；
    The quartzy monitoring method of amendment according to claim 5 prepares the method for broadband anti-reflection film deposition errors at the beginning of the thickness Beginning design load is modified, and the monitoring thickness of quartzy monitor is used as using correction result；
    It is coated with substrate using ion beam assisted depositing technique, with the deposition of quartzy monitor monitoring film, is obtained required Broad-band transparence-increased membrane sample.
CN201710944000.0A 2017-09-30 2017-09-30 Method for correcting deposition error of broadband antireflection film prepared by quartz monitoring method Active CN107893216B (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110058343A (en) * 2019-04-16 2019-07-26 河南平原光电有限公司 A kind of short-pass optical filtering membrane preparation method based on multi-angle spectral measurement
CN111856637A (en) * 2020-08-13 2020-10-30 苏州宏策光电科技有限公司 X-ray-based multilayer film zone plate correction method and system
CN113881926A (en) * 2021-09-24 2022-01-04 中国科学院上海光学精密机械研究所 Method for improving deposition precision of optical film
CN116463588A (en) * 2023-04-23 2023-07-21 有研国晶辉新材料有限公司 Preparation method of infrared filter film and infrared notch optical element
CN116590683A (en) * 2023-05-05 2023-08-15 北京创思镀膜有限公司 Optical film, preparation method thereof and optical film element

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CN102620664A (en) * 2011-01-28 2012-08-01 中国科学院理化技术研究所 Method for detecting coating-thickness uniformity of optical coating machine
CN104849861A (en) * 2015-06-01 2015-08-19 中国科学院光电技术研究所 Method for preparing high-performance optical thin film
CN205944718U (en) * 2016-07-29 2017-02-08 杭州科汀光学技术有限公司 A dual wavelength reflection reducing coating and optical film thickness monitored control system for quasi -molecule laser

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CN102620664A (en) * 2011-01-28 2012-08-01 中国科学院理化技术研究所 Method for detecting coating-thickness uniformity of optical coating machine
CN104849861A (en) * 2015-06-01 2015-08-19 中国科学院光电技术研究所 Method for preparing high-performance optical thin film
CN205944718U (en) * 2016-07-29 2017-02-08 杭州科汀光学技术有限公司 A dual wavelength reflection reducing coating and optical film thickness monitored control system for quasi -molecule laser

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110058343A (en) * 2019-04-16 2019-07-26 河南平原光电有限公司 A kind of short-pass optical filtering membrane preparation method based on multi-angle spectral measurement
CN110058343B (en) * 2019-04-16 2021-08-17 河南平原光电有限公司 Preparation method of short wave pass filter film based on multi-angle spectral measurement
CN111856637A (en) * 2020-08-13 2020-10-30 苏州宏策光电科技有限公司 X-ray-based multilayer film zone plate correction method and system
CN113881926A (en) * 2021-09-24 2022-01-04 中国科学院上海光学精密机械研究所 Method for improving deposition precision of optical film
CN113881926B (en) * 2021-09-24 2022-06-28 中国科学院上海光学精密机械研究所 Method for improving deposition precision of optical thin film
CN116463588A (en) * 2023-04-23 2023-07-21 有研国晶辉新材料有限公司 Preparation method of infrared filter film and infrared notch optical element
CN116463588B (en) * 2023-04-23 2023-11-03 有研国晶辉新材料有限公司 Preparation method of infrared filter film and infrared notch optical element
CN116590683A (en) * 2023-05-05 2023-08-15 北京创思镀膜有限公司 Optical film, preparation method thereof and optical film element
CN116590683B (en) * 2023-05-05 2023-12-26 北京创思镀膜有限公司 Optical film, preparation method thereof and optical film element

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